US4874952A - Device for accelerated photo-aging of materials containing polymers - Google Patents

Device for accelerated photo-aging of materials containing polymers Download PDF

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Publication number
US4874952A
US4874952A US07/187,367 US18736788A US4874952A US 4874952 A US4874952 A US 4874952A US 18736788 A US18736788 A US 18736788A US 4874952 A US4874952 A US 4874952A
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Prior art keywords
aging
accordance
temperature
aqueous phase
vat
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Expired - Lifetime
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US07/187,367
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English (en)
Inventor
Rene Arnaud
Jean-Luc Gardette
Jacques Lamaire
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UNIVERSITE DE CLERMONT II
Laboratoire de Photochemie of Universite de Clermont II
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Laboratoire de Photochemie of Universite de Clermont II
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Assigned to UNIVERSITE DE CLERMONT II reassignment UNIVERSITE DE CLERMONT II ASSIGNMENT OF ASSIGNORS INTEREST. Assignors: ARNAUD, RENE, GARDETTE, JEAN-LUC, LEMAIRE, JACQUES
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
    • G01N17/004—Investigating resistance of materials to the weather, to corrosion, or to light to light

Definitions

  • the invention relates to a device for the accelerated photo-aging of materials containing polymers, which device enables measurement of their capability to resist the simultaneous action of ultraviolet radiation, temperature and oxygen in an aqueous or gaseous phase in order to analyze with a view to better understanding the phenomena of photodegradation and to determining the correlations between the life spans of said materials under accelerated photo-aging and under climatic aging.
  • An accelerated photo-aging device for polymers is known from French Patent No. 2 430 609, which comprises chamber in which a single lamp emits a narrow parallel beam of ultraviolet radiation which irradiates a group of test pieces mounted on a sample holder, which group is reciprocally moved in translation in a plane perpendicular to the axis of the beam.
  • the temperature of the chamber is regulated so as to maintain constant the temperature of the test pieces, by means of temperature sensors in direct contact with said test pieces.
  • Such a device has disadvantages which are bothersome in use. Firstly, the polymer test pieces are submitted only to localized and discontinuous exposure to ultraviolet radiation due to the reciprocating movement of the sample holder. In addition, due to its construction, this device allows the simultaneous irradiation of only a small number of test pieces. Finally, such a device enables irradiation only in a dry atmosphere and, consequently, does not enable the study of the phenomena of photodegradation in the presence of an aqueous phase.
  • the accelerated photo-aging of polymers must necessarily be representative of the most extreme climatic phenomena, that is, not only the physical aggressions due to natural light and variations in temperature must be taken into account, but also the chemical aggressions due to the presence of an aqueous medium and/or oxygen such as occurs when the materials produced from polymers are used in direct contact with these natural elements.
  • a first type of device comprises an enclosure in which is placed a radiation chamber provided at its central part with three 4.5 kW Xenon lamps arranged in a triangle, with each lamp being provided with selective reflecting flat metal mirrors for ultraviolet light, around which are arranged two coaxial quartz cylinders, comprising an annular volume in which a cooling fluid circulates. Placed between the enclosure and the ultraviolet radiation chamber there is a cylindrically shaped sample holder moved in continuous or alternating rotation.
  • the device is provided in the upper part of the enclosure with one to three sprinkler ramps fitted with three nozzles enabling the creation of a damp internal atmosphere and/or a sprinkling of water onto the test pieces.
  • the device contains means enabling the temperature within the enclosure to be regulated by means of the continuous measurement of a black body located therein and to automatically adjust the test piece sprinkling cycles.
  • a black body located therein and to automatically adjust the test piece sprinkling cycles.
  • Such a device is known by the trade name of XENOTEST 1 200 HERAEUS.
  • Another type of device sold under the trademark HERAEUS XENOTEST 250 T provided with means for the thermal regulation of the enclosure and means for spraying water and adjusting the cycles of the spraying according to the preceding technique, is provided with a parabola-shaped reflector with a vertical axis, whose source is provided with a low pressure Xenon burner fitted with a filter, with the test pieces being arranged flat on the horizontal floor of the enclosure which thus acts as the sample holder.
  • the temperature of the polymer samples is not measured in a precise manner because, in each device, the temperature of the enclosure containing the samples is regulated via the measurement of the temperature of a black body placed in said enclosure, which temperature, according to the radiation properties of said body, is always higher than that of the samples.
  • resistance probes are arranged on a small rule placed in direct contact with the sample holder so as to measure, as far as possible, the temperature of the samples.
  • the temperature measured by the resistance probes is different from that of the exposed materials.
  • the samples of polymer used in the second device are maintained in a fixed position. Since the radiation emitted cannot have a perfectly homogeneous distribution over the entire volume of the irradiation chamber, the result is that the incident light intensity received by the samples during the total time of their irradiation cannot be the same from one sample to another and that heterogeneous distribution of said intensity can cause inaccurate aging test results.
  • a more specific device which consists of a parallelepipedal enclosure on which is placed a prism-shaped assembly provided with eight fluorescent tubes producing ultraviolet radiation placed horizontally, four by four, along two concurrent surfaces of the prism-shaped assembly.
  • the samples to be irradiated are then arranged between the tubes and the two above-identified concurrent surfaces.
  • the space defined by said concurrent surfaces and the samples enables a natural circulation of ambient air for cooling.
  • this device is also provided with a water vat for the generation of water vapor.
  • the difference in temperature existing between the water vapor and the internal irradiated surface of the samples cooled at their external surface due to the circulation of ambient air is sufficient to cause condensation of that water vapor coming into contact with said internal surface.
  • the thermal gradient which is established within the thickness of the sample does not enable the temperature of the irradiated material to be determined.
  • the samples placed along the concurrent surfaces of the enclosure are maintained in a fixed position throughout the entire time of the experiments and cannot therefore receive an equal amount of radiation from, one sample to another.
  • this device is provided with light sources emitting energy in the range of 270 to 350 nm which includes a photon-rich zone (between 270 and 300 nm) which does not exist in the solar spectrum.
  • the short wavelengths can create unrepresentative phenomena of natural aging in the accelerated laboratory photo-aging tests, such as accelerated photopassivation or photodegradation phenomena.
  • a simulation of the effect of the water must be characterized by the presence of a film of water maintained in direct and permanent contact with the polymer throughout the irradiation, with the oxygen concentration of said water being controlled and maintained at a constant value.
  • the devices described above do not enable the presence of a film of water of a given thickness over the entire surface of the irradiated test piece to be permanently ensured.
  • test piece produced using a thin strip of very hygroscopic polyamide, subjected in a sequential manner to sprinkling by spraying in a photo-aging enclosure brought to a temperature of between 40 and 70° C. has a dry surface a few minutes after the end of the sprinkling.
  • the present invention provides an accelerated photo-aging device for materials containing polymers, enabling samples of said materials to be subjected to the simultaneous action of ultraviolet radiation, temperature and oxygen in an aqueous or gaseous phase for the purpose of being able to analyze and interpret the phenomena of photodegradation.
  • the device in accordance with the invention includes an external enclosure which is polyhedral or possibly cylindrical in shape and having a vertical axis of symmetry, at least four sources of ultraviolet radiation evenly distributed at the periphery of the external enclosure and each emitting a beam of radiation in a selected wavelength range, at least one cylindrical wall which is transparent to radiation having a wavelength at least equal to 295 ⁇ 5 nm and which is coaxial to the external enclosure, a sample holder arranged coaxially to the vat and moved uniformly in rotation around its vertical axis, means circulating an aqueous phase inside the cylindrical wall, means regulating the temperature of the aqueous phase, means for saturating in oxygen the aqueous phase, means, for circulating a gaseous phase inside the external enclosure, and means for regulating the temperature of the exposed samples.
  • an external enclosure which is polyhedral or possibly cylindrical in shape and having a vertical axis of symmetry
  • the device in accordance with the invention comprises, as has been indicated, at least one cylindrical wall which is transparent to radiation having a wavelength at least equal to 295 ⁇ 5 nm, said wall being coaxial to the external enclosure of the device.
  • the device is provided with at least one and preferably two parallel cylindrical walls constituting the lateral walls of a crown-shaped vat which is closed in its lower part and open in its upper part, the hollow central part of which permits the axial placing of the sample holder.
  • the annular space in which the samples suspended on the sample holder are placed has a constant cross-section and enabled a volume of liquid with a controlled thickness to be maintained continuously in contact with the sample which can be partially and/or totally immersed in said liquid.
  • the distance between the two parallel cylindrical walls is such that it guarantees the existence of a film of water on the samples. This distance is between 5 and 50 and preferably between 10 and 30 millimeters.
  • These walls are generally produced of an optical material such as borosilicate glass which is transparent to ultraviolet radiations having wavelengths at least equal to 295 ⁇ 5 mn.
  • the sample holder In order that the samples undergo a very homogeneous irradiation, the sample holder is moved in a uniform rotation movement at a slow speed so that each sample moving evenly throughout the entire irradiation on the perimeter of the cylindrical wall receives a same amount of light flux.
  • the device in accordance with the invention is also provided with a means placed outside of the enclosure which continuously circulates the aqueous phase in the annular space of the crown shaped vat.
  • the temperature of said aqueous phase is regulated to a value selected by the skilled artisan using any known means such as a heat exchange or thermostat. This temperature thus enables the temperature of the samples to be fixed and controlled in a very precise manner.
  • the oxygen present in the aqueous phase is consumed in whole or in part by a photochemical reaction on contact with the polymer.
  • This oxygen must be renewed in such a manner that its concentration in the aqueous phase in contact with the samples remains approximately constant over time.
  • a suitable means such as for example one providing energetic stirring or blowing of air or oxygen, placed outside the enclosure, enables the oxygen, placed outside the enclosure, enables the oxygen content of the circulating aqueous phase to be maintained at its saturation point.
  • the sources emitting ultraviolet radiation are arranged in an even manner on the periphery of the external enclosure.
  • Said sources are preferably average pressure mercury vapor arc lamps emitting a photon-rich light with wavelengths of between 290 and 450 nm.
  • the shortest distance between the burner of one lamp and a sample can be selected in the range of 7 to 50 centimeters, and preferably close to 20 centimeters. This preferred range is adopted by the skilled artisan with a view to increasing the efficiency of the ultraviolet radiation and thus shortening the length of exposure time of the samples by increasing the photodegradation acceleration factor.
  • the number of sources emitting ultraviolet radiation is generally at least four. However, it may be more in order to provide an increase in the light flux and, consequently, to cause an increase in the speed of photo-oxidation.
  • the increase in the number of emitting sources for example from four to six emitting sources, enables the acceleration factor of the aging device to be increased, especially when the permitted temperature is greater.
  • the temperature existing inside the external enclosure, that is in the gaseous phase is controlled and regulated in relation to an average reference value, for example that of a temperature probe in contact with a reference sample which is not immersed in the aqueous phase and is representative of all the simultaneously irradiated samples.
  • the device in accordance with the invention contains at least two and preferably at least three ventilators for the introduction of air and at least one ventilator for the removal of air, which are provided on the walls of the external enclosure.
  • the starting up and stopping of these ventilators is controlled by any means known to the skilled artisan, such as a regulator comparing the measured temperature with that of a reference temperature. It is thus possible to maintain the temperature of the gaseous phase contained in the enclosure at the reference value by introducing into the enclosure fresh air taken from the outside atmosphere and, at the same time, removing the hot air.
  • the temperature of the samples in the gaseous phase which are being exposed is thus controlled and regulated using this reference value by means of said temperature probe.
  • the samples are immersed in the aqueous phase, their temperature is controlled and regulated using a reference value by the temperature of the circulating water.
  • the sample holder is composed of three main components, which are a shaft, a means for driving in rotation and at least one plate.
  • the shaft is positioned vertically and coaxially to the axis of the vat. It is provided at its lower end with a means for driving it in rotation and at it supper end with a circular plate which has a diameter substantially equal to that of the crown.
  • Means for fixing the samples are arranged at regular intervals on the periphery of the circular plate. Each sample is thus suspended from the plate in a vertical position, with its lower end able to remain free.
  • weights having a given value can be fixed on the lower part of each sample so as to maintain them under controlled traction throughout the irradiation time. It is thus possible to carry out the photo-aging study of polymers under traction, so as to cause premature degradation of the mechanical properties of the samples irradiated in this manner.
  • each sample can be inserted into a suitable support suspended on the circular plate.
  • the sample holder can be provided with a second plate located between the driving means and the upper plate and capable of sliding on the shaft.
  • the speed of rotation of the sample holder is generally selected in the range of 1 to 8 and preferably 3 to 5 revolutions per minute.
  • FIG. 1 is a schematic elevation view of a device according to the invention
  • FIG. 2 is a cross-section of the device along line II--II in FIG. 1.
  • the device shown in FIGS. 1 and 2 includes an external envelope (1) which, as shown in FIG. 2, has a cylindrical shape but which in accordance with the invention may have any other shape comprising a body of revolution around a vertical axis, such as a polyhedron.
  • a doubled-walled vat (2) is positioned in the enclosure and is made of a material transparent to radiation having a wavelength of at least 295 ⁇ 5 nm.
  • An aqueous phase circulates in the annular space defined by the two cylindrical walls of the vat. The upper end of the annular space is open so as to enable the insertion therein and the rotation of the samples (3).
  • Small tubes (4) and (5) connected vat (2) are in turn connected to suitable means (100) located outside the enclosure, for example means including a pump, a heat exchanger and an oxygen generator, which continuously circulates the liquid phase in the annular space of the vat (2), while maintaining a temperature and an oxygen concentration which are regulated to desired values.
  • a sample holder is composed of a shaft (6) provided at its lower part with a means (7) such as a pulley enabling it to be driven in rotation.
  • the upper part of shaft (6) is connected to a plate (8) having jaws (9) on its upper part on which sample holders are fixed and into which the samples (3) are inserted.
  • An assembly of four average pressure mercury vapor lamps (10) emitting photon-rich ultraviolet radiation having wavelengths at least equal to 295 ⁇ 5 are evenly distributed around the vat.
  • An assembly of three ventilators (11) driven so as to provide the introduction of fresh air are arranged on the lateral walls of the enclosure.
  • a fourth ventilation (12) driven so as to provide the removal of the hot air, is placed on the cover of the enclosure.
  • the starting up and the stopping of these ventilators is controlled by an electronic temperature regulator (200) in response to the measurement of the temperature of a reference sample which is not immersed in the liquid phase, the measurement being made by means of a thermometric sensor (210) such as a platinum probe or thermocouple.

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  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Ecology (AREA)
  • Biochemistry (AREA)
  • Environmental Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • Biodiversity & Conservation Biology (AREA)
  • Immunology (AREA)
  • General Physics & Mathematics (AREA)
  • Pathology (AREA)
  • Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)
  • Optical Fibers, Optical Fiber Cores, And Optical Fiber Bundles (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Polymerisation Methods In General (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Sampling And Sample Adjustment (AREA)
US07/187,367 1987-04-28 1988-04-28 Device for accelerated photo-aging of materials containing polymers Expired - Lifetime US4874952A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8706216A FR2614699B1 (fr) 1987-04-28 1987-04-28 Dispositif de photovieillissement accelere de materiaux contenant des matieres polymeres
FR8706216 1987-04-28

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US (1) US4874952A (de)
EP (1) EP0289436B1 (de)
AT (1) ATE107772T1 (de)
DE (1) DE3850298T2 (de)
FR (1) FR2614699B1 (de)

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US5111689A (en) * 1991-10-07 1992-05-12 The United States Of America As Represented By The Secretary Of The Army Background illumination simulator
US5136886A (en) * 1990-11-06 1992-08-11 Atlas Electric Devices Co. Accelerated weathering and lightfastness testing chamber
US5185532A (en) * 1991-05-21 1993-02-09 Oral Card Products Dental instrument sterilizer
US5220840A (en) * 1990-11-06 1993-06-22 Atlas Electric Devices Co. Method of calibrating light output of a multi-lamp light fastness testing chamber
DE4407608A1 (de) * 1994-03-08 1995-09-14 Dieter Dr Kockott Vorrichtung und Verfahren zur quantitativen Bewertung des Alterungsverhaltens eines polymeren Werkstoffes
WO1997027465A1 (en) * 1996-01-23 1997-07-31 American Home Products Corporation Light stability chamber
DE19632349C1 (de) * 1996-08-10 1998-01-08 Dieter Dipl Phys Dr Kockott Verfahren zur Bestimmung von Eigenschaftsänderungen einer Probe
US5854433A (en) * 1996-11-08 1998-12-29 Atlas Electric Devices Co. Variable rotation and irradiation weathering testing machine
US6546820B1 (en) * 2000-02-11 2003-04-15 Ann F. Koo Method and apparatus for multifunction vacuum/nonvacuum annealing system
US6611324B1 (en) * 2000-07-28 2003-08-26 Trw Inc. Method for testing solar cell assemblies by ultraviolet irradiation for susceptibility to ultraviolet degradation
US6682932B2 (en) 1998-09-24 2004-01-27 Kabushiki Kaisha Toyota Chuo Kenkyusho Weathering test method
US20040231440A1 (en) * 2000-12-13 2004-11-25 Beraud Michel Pierre Paul Accelerated artificial weathering test systems
US20050042759A1 (en) * 2003-02-28 2005-02-24 Basf Corporation Test method for determining etch performance of coated substrate
EP1517132A1 (de) 2003-09-18 2005-03-23 Atlas Material Technology GmbH Kontaktlose Messung der Oberflächentemperatur von natürlich oder künstlich bewitterten Proben
US6990868B2 (en) 2002-11-15 2006-01-31 Atlas Material Testing Techology Llc Accelerated weathering apparatus having sealed weathering chamber
US20060169037A1 (en) * 2005-01-31 2006-08-03 Atlas Material Testing Technology L.L.C. Temperature reduction fixture for accelerated weathering test apparatus
US20070051906A1 (en) * 2003-09-24 2007-03-08 Brennan Patrick J Method and apparatus for determining the resistance of materials to light and corrosives
US20080156120A1 (en) * 2006-12-28 2008-07-03 Cutriembres Fonseca S.A. Apparatus and Method for Testing Materials Exposed to Sunlight
US20100073011A1 (en) * 2008-09-23 2010-03-25 Applied Materials, Inc. Light soaking system and test method for solar cells
DE102009000179A1 (de) * 2009-01-13 2010-07-15 Evonik Degussa Gmbh Schnelltest zur Ermittlung des Einflusses einer Bestrahlung auf den Abrieb eines Granulats
DE102009000177A1 (de) * 2009-01-13 2010-07-15 Evonik Degussa Gmbh Schnellbestrahlungstest für Granulate
CN101968478A (zh) * 2010-08-27 2011-02-09 华南理工大学 医用镁合金生物降解性能体外动态模拟测试设备
CN101975738A (zh) * 2010-08-27 2011-02-16 华南理工大学 镁合金医疗器械生物降解性能体外动态模拟测试设备
CN102162787A (zh) * 2010-12-29 2011-08-24 常州亿晶光电科技有限公司 双面同时辐射测试的紫外老化试验箱
CN102323203A (zh) * 2011-05-30 2012-01-18 浙江华电器材检测研究所 用于复合材料芯棒光照老化试验的测试装置
US20150068328A1 (en) * 2013-09-06 2015-03-12 Atlas Material Testing Technology Gmbh Weathering testing having a plurality of radiation sources which are independently operable of one another
CN104713818A (zh) * 2013-12-17 2015-06-17 甘肃金海新材料有限公司 更换和维护防沙网的方法和防沙网的评估方法
CN105510216A (zh) * 2016-02-04 2016-04-20 郑州大学 便于搬运试样的大尺寸碳化池
CN105910979A (zh) * 2016-04-20 2016-08-31 上海林频仪器股份有限公司 一种光伏紫外试验箱
CN106353246A (zh) * 2016-10-21 2017-01-25 山西省交通科学研究院 一种沥青自动取样的多功能老化实验装置及其实验方法
CN107907405A (zh) * 2017-12-30 2018-04-13 广州市白云化工实业有限公司 结构密封胶加速老化装置及结构密封胶加速老化方法
CN111948123A (zh) * 2020-08-19 2020-11-17 江苏新源太阳能科技有限公司 一种电池组件老化检测装置
US11460393B2 (en) * 2019-06-27 2022-10-04 The Insulating Glass Certification Council System and method for accelerated weathering testing of insulating glass units

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FR2798733B1 (fr) * 1999-09-16 2001-11-16 Sud Hi Tech & Produits Procede de vieillissement solaire accelere et dispositif permettant l'application de ce procede
FR2826118B1 (fr) * 2001-06-14 2004-01-09 Michel Pierre Paul Beraud Dispositif d'exposition a des rayonnements photoniques pour des essais de vieillissement artificiel accelere d'echantillons
WO2002075283A1 (fr) * 2001-03-15 2002-09-26 Solsys Procede de vieillissement solaire accelere et dispositif permettant l'application de ce procede
CN103163062A (zh) * 2011-12-09 2013-06-19 海洋王照明科技股份有限公司 灯具材料老化测试电路、装置及方法

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Cited By (50)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5136886A (en) * 1990-11-06 1992-08-11 Atlas Electric Devices Co. Accelerated weathering and lightfastness testing chamber
US5220840A (en) * 1990-11-06 1993-06-22 Atlas Electric Devices Co. Method of calibrating light output of a multi-lamp light fastness testing chamber
US5185532A (en) * 1991-05-21 1993-02-09 Oral Card Products Dental instrument sterilizer
US5111689A (en) * 1991-10-07 1992-05-12 The United States Of America As Represented By The Secretary Of The Army Background illumination simulator
DE4407608A1 (de) * 1994-03-08 1995-09-14 Dieter Dr Kockott Vorrichtung und Verfahren zur quantitativen Bewertung des Alterungsverhaltens eines polymeren Werkstoffes
WO1997027465A1 (en) * 1996-01-23 1997-07-31 American Home Products Corporation Light stability chamber
US5660794A (en) * 1996-01-23 1997-08-26 American Home Products Corporation Light stability chamber
DE19632349C1 (de) * 1996-08-10 1998-01-08 Dieter Dipl Phys Dr Kockott Verfahren zur Bestimmung von Eigenschaftsänderungen einer Probe
US5854433A (en) * 1996-11-08 1998-12-29 Atlas Electric Devices Co. Variable rotation and irradiation weathering testing machine
US20040031336A1 (en) * 1998-09-24 2004-02-19 Kabushiki Kaisha Toyota Chuo Kenkyusho Weathering test method and apparatus
US6682932B2 (en) 1998-09-24 2004-01-27 Kabushiki Kaisha Toyota Chuo Kenkyusho Weathering test method
US6709631B2 (en) 1998-09-24 2004-03-23 Kabushiki Kaisha Toyota Chuo Kenkyusho Weathering test apparatus
US7018586B2 (en) 1998-09-24 2006-03-28 Kabushiki Kaisha Toyota Chuo Kenkyusho Weathering test apparatus
US6546820B1 (en) * 2000-02-11 2003-04-15 Ann F. Koo Method and apparatus for multifunction vacuum/nonvacuum annealing system
US6611324B1 (en) * 2000-07-28 2003-08-26 Trw Inc. Method for testing solar cell assemblies by ultraviolet irradiation for susceptibility to ultraviolet degradation
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EP0289436A3 (en) 1989-09-13
FR2614699A1 (fr) 1988-11-04
DE3850298D1 (de) 1994-07-28
FR2614699B1 (fr) 1989-06-09
DE3850298T2 (de) 1994-09-29
EP0289436B1 (de) 1994-06-22
ATE107772T1 (de) 1994-07-15

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